Process of making acetylene tetrachlorid.



No.x 804,516. .PATENTED NOV., 14, 1905. P.. ASKENASY & M. MUGDAN. PROCESS 0F MAKING ACBTYLENB TETRACHLORID.

APPLICATION FILED NOV. 10, 1903.

www' fwmwwwwwfy sAJrs r rn PAUL ASKENASY AND MARTIN MUGDAN, OF NUREMBERG, GERMANY.

PROCESS OIF WIKIING CETYLENE TETHACHLORID.

Specification of Letters Patent.

Patented Nov. 14, 1905.

Application iiled November 16, 1903 l Serial No. 181,410.

To all when?, t www concern:

Be it known that we, PAUL AsKnNAsY and MARTIN MUGDAN, subjects of the German Emperor, and residents of Nuremberg, Bavaria, German Empire, have invented a new and use- Yful Process of and Apparatus for Producing Tetrachlorid of Acetylene, of which the following is a description.

As is known, the action of acetylene on pentachlorid otl antimony produces compounds which are violently decomposable and from which compounds of acetylene and chlorin may be split ott (Acetylendi and Tetra chlorid, Berthelot and Junglleisch, Amm- /c/n. der U/wcrn/z'e uml IVW/wt., Vll. Suppl., 187 0, page Q52 and following pages.) A second method of producing tetrachlorid ot' acetylene is based on the action ot chlorin on acetylene with the aid of chlorid ot' aluminium dissolved in acetylene chlorid or tetrachlorid ol carbon, in connection with which process, however, it is absolutely necessary to exclude the very smallest quantity of air in order to avoid explosions. (Mouncyrat.) Many experiments have also been made with and without the aid of a cheap or indestructible intermediate substance to combine acetylene and chlorin without danger; but these experiments have hitherto had no technically exploitable result.

The process forming the object of the present invention enables the cheap and convenient production of acetylene tetrachlorid without danger and with a very slight loss of the intermediate substance.

Acetylene is .fed into pentachlorid ot' antimony which should advantageously contain no free chlorin. The pentachlorid of antimony may be diluted with a suitable medium, such as tetrachlorid of acetylene. In the first place the compound described by Berthelot and Junglieisch will be formed, which compound melts at about 50O centigrade. This compound, however, as we have tound,in contradistinction to Berthelots statement, will on further treatment with acetylene take up a second molecule of the gas. Berthelot and Jungfleisch heated the double compound of bichlorid ot' acetylene and pentachlorid of antimony with a surplus of the latter, (last cited page, 255, at the top.) We, however, leed chlorin into the product obtained from pentachlorid of antimony and acetylene, four atoms oiI the chlorin being bound by each molecule ot acetylene present, tetrachlorid or' acetylene being .formed and pentachlorid of antimony beingre-formed. Acetylene is then fed into the same'liuid, and then again chlorin, and so on alternately until, finally, it suilicient chlorin is fed, a mixture of pentachlorid or' antimony, tetrachlorid of acetylene, and small quantities of the products of substitution of the latter body is obtained. It the pentachlorid of antimony is diluted to avery great extent by the tetrachlorid ot acetylene produced, the reactions will still tale place .with sutlcient speed for economical purposes.

In order to isolate the tetrachlorid of acetylene, the pentachlorid otl antimony may be decomposed-for instance, by means of hydrochloric acid. It is, however, advantag'eous to subject the product ol the reaction to a slow fractionated distillation, in which case the pentachlorid of antimony changes to trichlorid of antimony by splitting otl the chlorin for thc most part, partly as escaping gas, partly by chlorinating the tetrachlorid ol acetylene to pcnta or hexa chlorethane. The trichlorid of antimony, which has a very high boiling-point, (2200,) may be easily separated from the tetrachlorid of acetylene, which boils at 1460.

The following are the details ot' a set of experiments: Two thousand nine hundred and seventy grams 10 molecules) SbCl absorbed consecutively four hundred and sixty six grams 18 molecules) C2H2 and two thousand iive hundred grams (-71 atoms) Cl, then four hundred and lii'ty grams (-17.3 molecules) (32H2 and two thousand three hundred and ten grams (-65.5 atoms) Cl, then three hundred and seventy grams 14. 2 molecules) C2H2 and eighteen hundred and ninety grams (-53.5 atoms) Ul, then two hundred and eighty grams (-10.8 molecules) C2H2 and seventeen hundred and sixty grams (-49.8 atoms) Cl, then three hundred and twenty grams (-12.3 molecules) C2H2 and two thousand one hundred grams (-59.5 atoms) Cl. About halt' the liquid obtained (seven thousand six hundred and fifty grams) was subjected to fractionated distillation during which at lirst chlorin and hydrochloric acid escaped. At a temperature above 215O centigrade eight hundred and sixty grams-vf. e. seventy-six per ccnt.- of the theoretical quantity of trichlorid of antimony distilled over. From the part which distilled below 1118O centigrade live thousand nine hundred grams of crude tetrachlorid oit acetylene could be obtained. The trichlorid of antimony after having been converted into pentachlorid was lit for use Ytor a new operation.

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The chlorin and acetylene may also be fed in simultaneously; but in this case they should In enter the apparatus at different points. this case the apparatus inust be constructed in the first place so that the two gases do not corne into contact with each other in order to avoid explosions,and, secondly, so that the absorbent liquid may circulate in order that the liquid treated with acetylene may come into contact with that treated with chlorin before the former is saturated, and vice versa.

In the accompanying drawing one forrn of apparatus is illustrated in the forrn of a diagram.

Chlorin pipe t and acetylene fiowsinto the bell G2 through the pipe f2. The liquid is intimately mixed with the gases by means of the stirrers R' and R2. The heat generated by the reaction is taken o in the cooling-coils K and K2. The liquid circulates through the two orifices L in the partition-wall Z.

Acetylene tetrachlorid is particularly suited on account of its cheapness for extracting fat, dissolving resins, oils, and the like.

IVe claiin as our inventionl. A process for producing tetrachlorid of flows into the bell G through the i acetylene, which consists in treating chlorid of antimony with acetylene and chlorin and then separating the tetachlorid of acetylene from the resulting productby fractionation, substantially as described.

2. A process for producing tetrachlorid of acetylene, which consists in treating the product of the reaction of acetylene and chlorid of antimony with clilorin and acetylene and then separating the tetrachlorid of acetylene froml the resulting product by fractionation, substantiall y as described.

3. A process for producing' tetrachlorid of acetylene, which consists in treating the product of the reaction of acetylene and chlorid of antiinony with chlorin and acetylene alternately and then separating the tetrachlorid of acetylene from the resulting product by fractionation substantially as described.

In witness whereof we have hereunto set our hands in presence of two witnesses.

PAUL ASKENASY. MARTIN MUGDAN.

Titnessesz LUDWIG SCUNINGEP., ALBERT BEsoLD. 

